DR.

MGR EDUCATONAL AND RESEARCH INSTITUTE

III Year V SEMESTER
ANALYTICAL INSTRUMENTS(BIC 301)

Two marks Questions & Answers

UNIT -I
PH and conductivity meters

1. How measurements are done in ion selective electrodes?

Ion selective electrodes measure ion activities, .ie. measures the thermodynamically
effective free ion concentration. In dilute solutions, ion activity usually approaches
ion concentration.

2. Define conductivity of electrolyte?

The conductivity of electrolyte is a measure of the ability of the solution to carry
electric current. The current through the solution takes place through the movement of
electrically charged particles called ions.

3. Why temperature compensation necessary in conductivity measurement?

The conductivity of electrolytic solution varies with temperature.this is because,
the ionic mobilites are temperature dependent. the temperature coefficient is of
the order of 1.5 to 2% at room temperature. So control of temperature is very
essential.

4. Give the methods of measurements of Oxygen?

Methods used to measure Oxygen are classified as either Physical or Chemical
methods . Physical method uses the paramagnetic property of Oxygen or
thermal conductivity as the basis for quantitative determination. Chemical
method includes potentiometric & catalytic combustion.
.

5. Give the application of Silica analyzer ?

In thermal power plants, silica content is measured in steam before turbine.
Silica analyzers are used for anion exchanger ,effluent monitoring & effluents
of mixed bed exchangers.

6. What are the two measurements made in Silica analyzer?

Chemical blank measurements
Quantitative determination

7. What is the use of blank in silica analyzer?

The reason for the use of blank on each cycle is to give the analyser long term
stability by compensating for the effect of variables such as coloration of the
sample or reagents, temperature,or aging of the lamp of photo cell.

8. Give the application of Sodium analyzer?

Sodium analysers find applications in thermal power plants for determining
sodium ion concentration in boiler water , monitoring carry over detection of
condenser leakes &the exhaustion of water treatment plant cation exchange
units.

9. Why ammonia gas is added to the sample in Sodium analyser?

The sodium selective glass electrode carries out the measurement in buffered
solution above 10PH , where it responds specifically to value of the sample is
sodium ion activity . So the PH must be adjusted to with in desired range .The
PH value of the sample is maintained in the flow cell by adding ammonia gas to
the sample.

10. Define humidity &Dew point?

Humidity is the measure of water vapour present in a gas.It is usually measured
as absolute humidity,relative humidityor dew point temperature.
Dew point is the temperature at which saturation of water vapour pressure
is equal to the partial pressure of water vapour in the atmosphere.

UNIT II
GAS ANALYSER

1. Define Thermal Conductivity of a gas?

Thermal Conductivity of a gas is defined as the quantity of heat (in
calories) transferred in unit time (seconds) in a gas between two surface 1 cm2 in
area when the temperature difference the surfaces is 1C.

2. What are the applications of thermal conductivity gas analyzer?

a. It is used in the measurement of hydrogen in blast furnace gases
b. In the determination of argon in Oxygen in the process of air
decomposition
c. In the determination of sulphur dioxide in roasting gases in the
production of sulphuric acid.

3. How is nitrogen-di-oxide prepared by chemiluminescence?

The nitric oxide reacts with ozone to form nitrogen-di-oxide with
chemiluminescence .
NO + O3 ----> NO2 + hv (light 0.6-3)

4. What are the advantages of Hydrogen Sulfide analyzer?

i) It do not require pumps or aspirators to pull in the sample
ii) They are unaffected by wind or variations in relative humidity.

5. What is the principle of H2S analyzer?

Sample at a constant flow rate enters a humidifier where it bubbles through
a 5% acetic acid solution. The sample then flows into the reaction window of the
sample chamber, where it passes over an exposed surface of paper sensing tape
impregnated with lead acetate. H2S reacts with lead acetate to form lead sulfide
causing a brown stain on the paper. The rate of reaction and resulting rate of color
change is proportional to the concentration of H2S in the sample.

6. What is the principle of CO analyzer?

It is based on the oxidation of carbon monoxide. It is oxidized by hot
mercuric oxide. CO + HgO ----> CO2 + Hg(g)
The mercury vapor released may be measured photometrically.

7. What is the use of protective filter in Industrial analyzer?

In Industrial analyzer gas-handling components should always include a small protective
filter, preceded by a major filter if the gas contains suspended matter
that requires removal.

8. What are the applications of oxygen analyzer?

i) It is used in the areas of oxygen absorption studies on plants and tissues
.ii) It is used in food processing industries.
iii) It is also used in respiratory studies.

9. Explain the detection methods of Carbon Monoxide Analyzer?

i) Non dispersive method
ii) Mercury Vapour
iii) Catalytic Oxidation
iv) Electrochemical fuel cell

10. What is necessity of converting nitric oxide to nitrogen-di-oxide?

This is because nitric oxide is essentially transparent in the visible and
ultraviolet regions, it must first be converted to NO2 before it can be measured

Unit III
CHROMATOGRAPHY

1. Define chromatography.
Chromatography is defined as the physical and chemical method of seperation
between various components of a mixture into pure fractions or bands of each
component.

2. What are the different types of gas chromatography?

The different types of gas chromatography are
Gas liquid chromatograpry
Gas solid chromatography.

3. What are the different parts of gas chromatography?

Carrier gas supply with regulators,gauges and flow meters
Sample injection system
Chromatographic column
 Thermostat
Detector
Recorder.

4. Give the selection criteria for carrier gas.

The selection criteria for carrier gas are
It should be very cheap
It should have high thermal conductivity
It should be inert
The carrier gas should be selected according to the type of
detector used.

5. Write short notes about gas chromatographic column.

The column acts as the heart of a gas chromatography, where the fundamental
process of separation takes place. Its action is based on the fact that when a sample of
gas or vapour is introduced into the column, it spreads by molecular diffusion to give a
concentration profile.As the sample moves through the column, additional spreading
takes place. But, the band maintains the general shape, which is detected and recorded
as a chromatographic peak.
The chromatographic columns are of two types as
Packed column
Capillary or Open tubular column.

6. List some detectors in gas chromatography .

Thermal conductivity detector
Flame ionization detector
Thermionic emmision detector
Electron capture detector
Flame photometer detector
Photo ionization detector
Electrolytic conduction type of detection
Dual detector

7. Give the principle of Gas-Liquid chromatography.

If the vapour or gas comes in contact with a liquid, a fixed amount of it gets
dissolved in the liquid. This takes place according to Henryslaw of partion given by
x /m =kc
where m mass of liquid used
c vapour concentration in the gas phase
x mass of gas
k constant .

8. Write the features of thermal conductivity detector .

It is simple, inexpensive, non-selective and non destructive and displays a
universal responce
Being non destructive ,the column effulent can be passed through a TCD and
then into a second detector
The sensitivity is 0.3 ng/ml . The linearty is between 104 to 105
It is particularly suitable for fraction correction and preparative gas
chromatography
.
9. Write the limitations of gas chromatography .
Only about 20% of known compounds lend themselves to analysis by gas
chromatography . This is because the compounds are volatile and they cannot pass
through the column. Also they are thermally unstable and decompose under certain
conditions of seperation.

10. What are the different types of liquid chromatography?

The different typesof liquid chromatography are
Liquid-liquid chromatography
Liquid-solid chromatography
Ion exchange chromatography or Bonded phase chromatography
Exclusion chromatography

UNIT IV
Spectrophotometers

1.State Lambert-Beer law.

The relation representing
Lnp0/p=kbc
Where p0 is the radiant power at distance&concentration=0.and
P is the radiant power at distance=b&concentration=c and
K is a constant is known as Lambert_Beer law.

2.State the major process involved in AAS.

The AAS phenomenon can be divided into two major process
1.The production of free atoms from the sample
2.The absorption of radiation from an external source by these atoms

3. Name the types of detectors used for IR spectrometry.

1.Thermal detectors in which the infrared radiations produces a heating effect that alters
some physical property of the detectors
2.Photon detectors

4.Define spectroscopy.
Spectroscopy is the measurement and interpretation of radiation
emitted,scattered or absorbed by different atoms,molecules & other chemical species
.
5. Name the different types of spectrophotometers.
1.UV_ vsible spectrophotometers.
2.Infrared spectrophotometers.
3.FIFR spectrophotometers.
4.Atomic absorption spectrophotometers.
5.Flame emission spectrophotometers

6.Give any two applications of flame emission spectrometry.

1.FES is used in the determination of trace metals in liquid samples.
2.FES finds wide application in agricultural and environmental analysis,industrial
analysis of ferrous metal and alloy as well as glasses .

7.Name few IR radiation sources.

1.incandescent source
2.nernst glower
3.globar source
4.mercury arc.

8.Give the advantages of grating monochromators

1.gratings can be made with materials like aluminium which are not affected by
moisture.
2.grating monochromators can be used over wide wavelength ranges

9.Specify the major design requirements of monochromators.

1.simplicity
2.resolution
3.spectral range
4.purity of exiting radiation
5.dispersion

10.State the principle of operation of flame emission spectrometry.

In FES the sample solution is nebulized and introduced into the flame
where it is desolvated,vapourized and atomized,all in rapid succession.
Subseqently,atoms and molecules are raised to excited states via thermal collisions with
the constituents of the partially burned flames gases.Upon their return to a lower or
ground electronic states the excited atoms and molecules emit radiation characteristic of
the sample components.

UNIT V
Nuclear magnetic Resonance and Radiation techniques.

1. Write any three applications of NMR Spectrometer. I.

Quantitative analysis :
The NMR Spectrometry is used to determine the molar ratio of
components in a mixture.
II. Hydrogen Bonding:
Here the NME is used to study Hydrogen bonding in organic
compounds proton signal is
shifted towards low field in the case of hydrogen bonding.
III. Elemental analysis:
Here NBMR Spectrometer is used for determination of the total
concentration of a given kind of magnetic nucleus in the sample.

2. Mention the limitations of NMR ,Spectrometer.

1. Lack of Sensitivity.
2. While charactersing the organic compounds, no information about the
molecular weight is given, but the relative number of different protons present
are only known.
3. In some compounds, two different types of H2 atoms at similar resonance
frequencies resulting in an overlap of spectra .This makes difficult
interpretation of such overlapped spectra.
4. In most of the cases,only liquids can be studied by NMR spectrometry.

3. What is Mass Spectrometry?

Mass spectrometry is the most commonly used method which provides qualitative and
quantative information about the atomic and molecular
composition of organic and inorganic materials.It produces charged particles that
consist of the parent ion and ionic fragments of the original molecule,and it sorts these
ions acording to their mass/charge ratio.

4. Mention the advantages of Mass spectrometry.

1.Better Sensitivity.
2. More detailed understanding of kinetics and mechanisms of
unimolecular decomposition of molecules.
3. Improved Speicificity in identifying unknowns or confirming the
presence of suspected components.

5. What are the various parts of the Mass spectrometer?

1.Sample inlet system.
2.Ion source.
3. Ion acceleration and Mass analyser.
4. Ion collection system
5.Data handling system.
6.Vaccum system.

6. How can we obtain the NMR absorption spectra?

NMR absorption spectra can be obtained either by changing
the freqauency of the Radio frequency oscillator or by changing the spacings of the
energy levels by varying the magntic field.

7. Define Absorption ,Fluorescence, Diffraction in X-ray Spectrometers?

Absorption of X-rays gives the information about the absorbing
material just as in other regions of the spectrum.
Fluorescence emission of X-rays enables to identify and measure
heavy elements in the presence of each other and in any matrix.
Diffraction of X-rays enables analysis of crystalline materials with
a high degree of specificity and accuracy.

8. What are the basic instrumentation of X-ray spectrometer

1.X-ray generating equipment
2.Collimator
3.Monochromator
4.Detector

9. Types of Nuclear radiation detectors:

1.Photo graphic Emulsions
2 .Ionization chamber
3.The Geiger counter
4.Proportional counter
5.Scintilation gounter
6. Semi conductor detector

10. Write short notes about the X-ray generating equipment ?

X-rays are generated in specially designed high vaccum sealedofff
tubes,which have copper or molybdenum as target.Targets are made of tungsten
,iron,chromium,nickel are also sometimes used for special purposes .Due to the
bombardment of electrons, under the influence of the high voltage, the target becomes
hot, which can either rotated or cooled with cooling water.

16 MARKS QUESTIONS
UNIT -I
PH and conductivity meters

1) Describe in detail about the constructional details and working principles of ion
selective electrodes.
Ref : Handbook of Analytical Instruments
-R.S. Khandpur
Page : 464 470

2) Define pH. What are the design criteria of pH meters? Explain anyone type of pH
meter in detail.
Ref : Handbook of Analytical Instruments
-R.S. Khandpur
Page : 448, 455 458

3) Explain with neat diagram a method of measuring oxygen dissolved in water.

Ref : Handbook of Analytical Instruments
-R.S. Khandpur
Page : 464 470

4) With neat diagram, explain in detail the principle of operation of sodium analyser.
Ref : Mechanical & Industrial Measurements
-R.K.Jain
Page : 846 848

UNIT II
GAS ANALYSER

1) With neat diagram, explain in detail the working principle of O2 Analyser based on
magnetic susceptibility.
Ref : Handbook of Analytical Instruments
-R.S. Khandpur
Page : 491 493

2) Draw & explain the shematic diagram of a NO-NO2 analyser.

Ref : Process Measurements and Analysis
-B.G.Liptak

3) With neat diagram, describe the working principle of a H2S analyser.

Ref : Process Measurements and Analysis
-B.G.Liptak

4) Explain in detail the principle of working of thermal conductivity

analyser with neat diagram.
Ref : Handbook of Analytical Instruments
-R.S. Khandpur

Unit III
CHROMATOGRAPHY

1) Draw the schematic diagram of a gas chromatograph & explain the components.
Ref : Instrumental methods of analysis
Willard, Meritt, Dean, Settle
Page : 540 544

2) Discuss any two types of detectors used in Gas Chromatography.

(i) Thermal conductivity detector
(ii) Flame ionization detector
Ref : Instrumental methods of analysis
Willard, Meritt, Dean, Settle
Page : 552 555

3) Draw & explain the instrumentation of HPLC in detail.

Ref : Instrumental methods of analysis
Willard, Meritt, Dean, Settle
Page : 592 596
4) Describe in detail any two types of detectors used in Liquid chromatography.
Ref : Instrumental methods of analysis
Willard, Meritt, Dean, Settle
Page : 600 607

UNIT IV
Spectrophotometers

1) Explain the single beam & double beam instruments used in UV spectrophotometer.
Ref : Instrumental methods of analysis
Willard, Meritt, Dean, Settle
Page : 148 154

2) What are non-dispersive spectrometers? Explain in detail the FTIR spectrometer. What
are the advantages of the same?
Ref : Instrumental methods of analysis
Willard, Meritt, Dean, Settle
Page : 301 305

3)Draw & explain the arrangement of the major parts of single beam & double beam
Atomic absorption spectrometer.
Ref : Instrumental methods of analysis
Willard, Meritt, Dean, Settle
Page : 243 246

4) Explain with neat diagram about Flame emission spectrometer.

Ref : Instrumental methods of analysis
Willard, Meritt, Dean, Settle
Page : 243 246

UNIT V
Nuclear magnetic Resonance and Radiation techniques.

1) What is the basic principle of NMR? Discuss the working principle of NMR
spectrophotometer & give its applications.
Ref : Instrumental methods of analysis
Willard, Meritt, Dean, Settle
Page : 422, 431 437

2) Describe the working principle of GM counter & proportional counter in detail.

Ref : Instrumental methods of analysis
Willard, Meritt, Dean, Settle
Page : 351 355

3) Draw the block diagram showing the major components of a Mass spectrometer &
describe.
Ref : Instrumental methods of analysis
Willard, Meritt, Dean, Settle
Page : 466 468

4) Explain the X-Ray spectroscopy in detail.

Ref : Handbook of Analytical Instruments
-R.S. Khandpur
Page : 324 329
 DR. MGR EDUCATONAL AND RESEARCH INSTITUTE
III Year V SEMESTER
ANALYTICAL INSTRUMENTS(BIC 301)

Two marks Questions & Answers

UNIT -I
PH and conductivity meters

1. How measurements are done in ion selective electrodes?

2. Define conductivity of electrolyte?
3. Why temperature compensation necessary in conductivity measurement
4. Give the methods of measurements of Oxygen?
5. Give the application of Silica analyzer ?
6. What are the two measurements made in Silica analyzer?
7. What is the use of blank in silica analyzer?
8. Give the application of Sodium analyzer?
9. Why ammonia gas is added to the sample in Sodium analyser?
10. Define humidity &Dew point?

UNIT II
GAS ANALYSER

1. Define Thermal Conductivity of a gas?

2. What are the applications of thermal conductivity gas analyzer?
3. How is nitrogen-di-oxide prepared by chemiluminescence?
4. How is nitrogen-di-oxide prepared by chemiluminescence?
5. What are the advantages of Hydrogen Sulfide analyzer?
6. What is the principle of H2S analyzer?
7. What is the use of protective filter in Industrial analyzer?
8. What are the applications of oxygen analyzer?
9. Explain the detection methods of Carbon Monoxide Analyzer?
10. What is necessity of converting nitric oxide to nitrogen-di-oxide?

Unit III
CHROMATOGRAPHY

1. Define chromatography.
2. What are the different types of gas chromatography?
3. What are the different types of gas chromatography?
4. Give the selection criteria for carrier gas.
5. Write short notes about gas chromatographic column.
6. List some detectors in gas chromatography .
7. Give the principle of Gas-Liquid chromatography.
8. Write the features of thermal conductivity detector .
9. Explain the detection methods of Carbon Monoxide Analyzer?
10. What is necessity of converting nitric oxide to nitrogen-di-oxide?

UNIT IV
Spectrophotometers

1 .State Lambert-Beer law.

2. What are the different types of gas chromatography?
3. Name the types of detectors used for IR spectrometry.
4. Define spectroscopy
5. Name the different types of spectrophotometers.
6. List some detectors in gas chromatography .
7. Name few IR radiation sources
8. Give the advantages of grating monochromators
9. Specify the major design requirements of monochromators
10. State the principle of operation of flame emission spectrometry.

UNIT V
Nuclear magnetic Resonance and Radiation techniques.

1. Write any three applications of NMR Spectrometer. I.

2. Mention the limitations of NMR ,Spectrometer.
3. What is Mass Spectrometry?
4. Mention the advantages of Mass spectrometry.
5. What are the various parts of the Mass spectrometer?
6. How can we obtain the NMR absorption spectra?
7. Define Absorption ,Fluorescence, Diffraction in X-ray Spectrometers?
8. What are the basic instrumentation of X-ray spectrometer
9. Types of Nuclear radiation detectors:
10. Write short notes about the X-ray generating equipment ?

16 MARKS QUESTIONS
UNIT -I
PH and conductivity meters

1) Describe in detail about the constructional details and working principles of ion
selective electrodes.
2) Define pH. What are the design criteria of pH meters? Explain anyone type of pH
meter in detail.
3) Explain with neat diagram a method of measuring oxygen dissolved in water.
4) With neat diagram, explain in detail the principle of operation of sodium analyser.

UNIT II
GAS ANALYSER

1) With neat diagram, explain in detail the working principle of O2 Analyser based on
magnetic susceptibility.
 2) Draw & explain the shematic diagram of a NO-NO2 analyser.
3) With neat diagram, describe the working principle of a H2S analyser.
4) Explain in detail the principle of working of thermal conductivity
analyser with neat diagram.

Unit III
CHROMATOGRAPHY

1) Draw the schematic diagram of a gas chromatograph & explain the components.
2) Discuss any two types of detectors used in Gas Chromatography.
3) Draw & explain the instrumentation of HPLC in detail.
4) Describe in detail any two types of detectors used in Liquid chromatography.

UNIT IV
Spectrophotometers

1) Explain the single beam & double beam instruments used in UV spectrophotometer.
2) What are non-dispersive spectrometers? Explain in detail the FTIR spectrometer. What
are the advantages of the same?
3)Draw & explain the arrangement of the major parts of single beam & double beam
Atomic absorption spectrometer.
4) Explain with neat diagram about Flame emission spectrometer.

UNIT V
Nuclear magnetic Resonance and Radiation techniques.

1) What is the basic principle of NMR? Discuss the working principle of NMR
spectrophotometer & give its applications.
2) Describe the working principle of GM counter & proportional counter in detail.
3) Draw the block diagram showing the major components of a Mass spectrometer &
describe.
4) Explain the X-Ray spectroscopy in detail.